反应详情

To a refluxing solution of 60A (1.7 g, 5.8 mmol), EtOH (60 mL), water (15 mL) and AcOH (4 mL) was added portion-wise Fe powder (1.63 g, 29.0 mmol) over 30 min. The mixture was heated for 45 min. before cooling to ambient temperature and filtered through celite. Filtrate concentrated in vacuo to afford 60B (1.5 g, 95%) as an oil. 1H NMR (400 MHz, CDCl3) δ ppm 1.25-1.41 (m, J=4.39 Hz, 3 H) 2.27 (s, 3 H) 2.61 (s, 2 H) 2.92 (s, 2 H) 4.22 (s, 2 H) 4.64 (s, 1 H) 6.84-7.56 (m, 12 H)

1. temperatureThe mixture was heated for 45 min.
2. filtrationfiltered through celite
3. concentrationFiltrate concentrated in vacuo